Yamini Yadollah, Safari Meysam, Shamsayei Maryam
Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
Department of Chemical Engineering, Kermanshah University of Technology, Kermanshah, Iran.
J Pharm Anal. 2018 Aug;8(4):250-257. doi: 10.1016/j.jpha.2018.05.005. Epub 2018 May 27.
The copper-coated iron oxide nanoparticles with core-shell were produced by deposition of a Cu shell on FeO NPs through reduction of Cu ions in solution using NaBH. Subsequently, the organosulfur compound, bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid (b-TMP-DTPA), was used to form self-assembled monolayer in order to modify sorbent's surface via covalent bonding between Cu and thiol (-SH) terminal groups. The prepared magnetic nanoparticles were characterized by using Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and thermo gravimetric analysis (TGA). Then, the application of this new sorbent was investigated to extract the steroid drugs in ointment samples with the aid of ultrasound. An external magnetic field was applied to collect the magnetic nanoparticles (MNPs). The extracted analytes were desorbed using acetonitrile. The obtained extraction solution was analyzed by HPLC-UV. The main affecting factors on the extraction efficiency including pH, sonication time, amount of sorbent, salt concentration, and desorption conditions were optimized in detail. Under the optimum conditions, good linearity was obtained in the range of 2.5-250.0 µg/ L with reasonable linearity (R > 0.99) and the limits of detection (LODs) ranged between 0.5 and 1.0 µg/L (based on S/N = 3). Repeatability (intra-day precision) based on five replicates and preconcentration factors were calculated to be 3.6%-4.7% and 87-116, respectively. Relative recoveries in ointment samples at two spiked levels of the target analytes were obtained in the range of 90.0%-103.2%. The results illustrated that the FeO@Cu@ b-TMP-DTPA NPs have the capability of extraction of steroid drugs from ointment samples.
通过使用硼氢化钠（NaBH）还原溶液中的铜离子，在FeO纳米颗粒上沉积铜壳，制备了具有核壳结构的铜包覆氧化铁纳米颗粒。随后，使用有机硫化合物双（2,4,4-三甲基戊基）二硫代次膦酸（b-TMP-DTPA）形成自组装单分子层，以便通过铜与硫醇（-SH）端基之间的共价键修饰吸附剂表面。使用傅里叶变换红外（FT-IR）光谱、扫描电子显微镜（SEM）、透射电子显微镜（TEM）、振动样品磁强计（VSM）和热重分析（TGA）对制备的磁性纳米颗粒进行了表征。然后，研究了这种新型吸附剂在超声辅助下提取软膏样品中甾体药物的应用。施加外部磁场以收集磁性纳米颗粒（MNP）。使用乙腈解吸提取的分析物。通过HPLC-UV对获得的提取溶液进行分析。详细优化了对提取效率的主要影响因素，包括pH值、超声时间、吸附剂用量、盐浓度和解吸条件。在最佳条件下，在2.5-250.0μg/L范围内获得了良好的线性，线性关系合理（R>0.99），检测限（LOD）在0.5至1.0μg/L之间（基于S/N=3）。基于五次重复计算的重复性（日内精密度）和预富集因子分别为3.6%-4.7%和87-116。在两种加标水平的目标分析物的软膏样品中的相对回收率在90.0%-103.2%范围内。结果表明，FeO@Cu@b-TMP-DTPA NPs具有从软膏样品中提取甾体药物的能力。
